Stannous Chloride → 8-Fluoro-2-methyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride

HRID 1350502노트

반응식

HRID 1350502 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][C:9]2[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][C:10]=2[C:11]#[N:12])=[C:4]([N+:18]([O-])=O)[CH:3]=1.[Sn](Cl)[Cl:22]>C(O)C.Cl>[ClH:22].[F:1][C:2]1[CH:7]=[CH:6][C:5]2[NH:8][C:9]3[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][C:10]=3[C:11]([NH2:12])=[N:18][C:4]=2[CH:3]=1

참가 물질

5

반응물 2

HCID 24479Stannous ChlorideHCID 210934602-(4-Fluoro-2-nitro-phenylamino)-5-methyl-benzonitrile

생성물 1

HCID 1357977618-Fluoro-2-methyl-5H-dibenzo[b,e][1,4]diazepin-11-ylamine hydrochloride수율 73%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 702Ethanol용매

실험 절차

Heat a solution of 2-(4-fluoro-2-nitro-phenylamino)-5-methyl-benzonitrile (1.747 g, 6.44 mmol) in ethanol (35 ml) to 60° C. and add a solution of tin (II) chloride (6.06 g, 31.96 mmol) in 5.0 N hydrochloric acid (35 ml). Reflux the resulting mixture to reflux for 40 hours. Cool the reaction to room temperature and place in a freezer for 16 hours. The product precipitates from the solution and is collected by filtration to obtain 1.3 g of the title compound (4.68 mmol, 73% yield) as a yellow-green amorphous solid: Mass Spectrum (m/e): 241 (M+1).

후처리

  1. temperatureReflux the resulting mixture
  2. temperatureto reflux for 40 hours
  3. temperatureCool
  4. customthe reaction to room temperature
  5. customThe product precipitates from the solution
  6. filtrationis collected by filtration

출처 및 근거

ORD 기록
ord-d4457e3887674d0a85f780eaf9558d2f
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214673B2

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